This paper reports the detail synthesis of a new kind of metal iodate, anhydrous (LiFe1 3)(IO3)(2), from aqueous solutions. The synthesized compound shows spinal morphology and is chemical stable up to 400:C. The iodate shows paramagnetic behavior from room temperature down to 4.2 K, At room temperature. the new compound has a hexagonal structure with the lattice parameters a = 5.4632(2) Angstrom, c = 5.0895(6) Angstrom, Z = 1, space group of P6(3). (C) 2002 Elsevier Science B.V. All rights reserved.